Process of purifying and decolorizing rosins with resorcinol



' adaptation of present known commercial Patented June 16, 1931 I terialby means of resorcinol.

rosins.

TES PATENT. OFFICE IVER 'GUBELMANN' AND CLYDE O. HENKE, OF SOUTHMILWAUKEE, WISCONSIN, AS-

SIGNORS TO THE NEWPORT COMBANY, OF CARBOLLVILLE, WISCONSIN, A. CORPORA-T103! OF DELAWARE y PROCESS OF PURIFYING AND DEQOLORIZING ROSINS WITHRESORCINOL No Drawing.

Application filed July 25, 1927. Serial No. 208,407.

vantage of by our improved method of purifying and decolorizing rosin.In general, our process comprises dissolving the rosin in a suitablesolventtherefor, and in treating the rosin solution thus selectivesolvents which are capable: of exformed with a relatively small quantityof tracting the impurities'and coloring matters resorcinol to extractrosin impurities and from the rosin. The selective solvents con-ocoloring matters. taining the i purities are then removed rosins areprepared by extracting finely comfrom the rosin solution and the rosinis reminuted resinous woods with various solcovered from the purifiedsolution. Ainon vents, of which some'of the better known are otherselective stilvents phenol (C H OH petroleum, naphtha, gasoline,turpentine and has been proposed.

This invention relates to a process of purifylng and decolor1z1ng rosincontaming ma- It has been proposed rosin by treating a I other cyclicand aliphatic hydrocarbons.

The-present invention-constitutes certain Practically any ofthesesolvents ,may be improvements over the said process, in that used 1n ourprocess provided that the solvent we have found. thatresorcinol'possesses many advanta es from a practical standpoint over atlow and ordinary temperatures. other p enolic solvents and lends itselfAfter the resorcinol has been added to the readily to a modification ofpresent rosin extraction methods; j

It is therefore an object of this invention to provide an improvedmethod of'purify-. ing and decolorizing rosins. by means of of theimpurit es and coloring matter by resorcinol wherein low grade resinsmay be the resorcinol has been-largely effected. The

converted to high grade ros'insby the simple mass is then cooled to atemperature at which the resorcinol solidifies. Ordinarily,

the resorcinol containing the impurities and coloring matter present inthe original rosin which adheres to the exsome of the resorcinol to anelevated temperature, that is, around methods for the extraction" ofcommercial object of this inventionto solidifies to a crust It ,isfurther traction apparatus,

provide a method of purifying and decolorizing rosins by 'means ofresorcinol, andjto also being pr Q P t0 the bOttOII"! 0f the provide asimple The solution of purified rosin method for recoveringthexapparatus.

resorcinol for re-use in subsequent opera-v may then be drawn offcompletely by detions. cantation without the difficulties usually atvOther and further important objects of tendant in making a separationbetween two this invention w1ll be apparent from the disliquid layers.

"closures in the specification and the append-- ered from its solutionby ordinary or steam ed claims.

I v distillation. has .a"sele ctivesolvent action The small amount ofresorcinol which is Resorcinol,

contained in the rosin solvent solution can toward the impurities andcoloring matters normally contained in wood and, gum rosins.

We ave now. found that resorcinol has to the very high water solubilitycertain other properties which-render its cinol and'to the very lowsolubility of'rebodies, such as phenol.

very low solubility in the common rosin solapplication to the purifying"of rosin more sorcinolin common rosin solvents. The advantageous thanthe use of other phenolic -'recovery of the resorcinol from this waterResorcinol has a solution will be described hereinafter.

The solid mass of resorcinol andextracted vents and it further hastheconvenient property of solidifying at ordinary temperatures,

both of which properties can'be'taken .adthe above separation may alsobe treated As is well known, wood rosin solution, the mass is preferablyheated 70 the boiling temperature of the rosin solvent, and efficientlyagitated until the'extraction The purified rosin is recov-- be extractedquantitatively with'water, due

of resor-- rosin impurities and coloring matter remainlng 1n theextractlon apparatus after used is relatively immiscible with resorcinolcient when used in connection with a com-- mercial solution of rosin,pine oil and other terpenes in a rosin solvent, as the solution 'isordinarily obtained in the production of rosin from resinous woods bypresent extractive methods.

Without limiting our invention to any particular procedure, thefollowing example, in which parts by weight are expressed illustrates anembodiment of our preferre method:

' To a solution of 2,000 parts of rosin ex tract, as it is commonlysecured in the production of wood rosin by extraction of resinous woodswith petroleum naphtha, are added 50 parts of resorcinol and theresulting mixture heated to boiling with eflicient agitation. themixture is then cooled to ordinary or low temperatures, say 15 C. withthorough "stirring. There results a solution of purified rosin and aprecipitated solid mass, from which the rosin solution may be easilydecanted. The so decanted solution contains, in addition to the purifiedrosin, a small amount of dissolvedresorcinol, which is then extractedwith water. The precipitatedsolid mass contains most of the resorcinol,which is treated in the extraction apparatus by boiling with water, bwhich method the resorcinol is practically completely extracted. Thewater solution of the resorcinol is-decanted from the residual coloringmatter and combined with the above mentioned water solution ofresorcinol. The combined resorcinol water so- .lutions are evaporated todryness in a still,

leaving solid resorcinol in the bottom of the still suitable for re-usein "subsequent operations. "Thearosin is recovered from the solventsolution in a highly purified form by the usual method.

According to the above method, either wood rosin or gum rosin may begreatly improved in grade,. and inferior grades of rosin suflicientlypurified for use in manufacturing processes requiring. the highestgrades of rosin. It should be noted that our method requires relativelysmaller quantities of resorcinol than where phenol is used as theselected solvent for the rosin impurities and coloring matter. It shouldalso be noted that where it is often desirable out departin Withoutprolonged treatment,

, the rosin solution from the resorcino 'itate.

and necessary to make moreflthan one extract when phenol is used as theselective We are aware that many changes may be made and numerousdetails of the process maybe varied through a wide range Withfrom'theprinciples of this invention, an we, therefore, do not purpose limitingthe patent (granted hereon, otherwise than necessitate by the prior art.

We claim as our invention:

1. In the process of purifying and decolsolvent, according to ourmethod, fewer extracts give highly satisfactory results.

orizing rosins, the steps which comprise treating a rosin dissolved in acommon rosin solvent with resorcinol at an elevated temperature, saidsolvent being relati'vel immiscible with resorcinol at lowand or inarytemperatures, and cooling to precipitate the resorcinol containingdissolved mpurities and coloring matter.

2.In the process of purifyin and decolorizing rosins, the steps -.Wl11Ctreating a solvent extraction mass from resinous wood containing rosin,pine oil and other terpeiies and a relatively volatile liquidhydrocarbon immiscible at low tem peratures with resorcinol, withresorcinol at an elevated temperature and CQ0l1Il l'/Q precipitate theresorcinol containing isso ved impurities and coloring matter.

3. In the process of purifyin' and decoloriz'ing rosins, the steps whiccomprise treating a rosin dissolved in a relatively v ol, atile liquidhydrocarbon. immisc ble with resorcinol at low and ordinarytemperatures, with resorcinol at an elevated temperature, coolingtoprecipitate the resorcinol containing-diss olved impurities and color ngmatter and separating the rosin solution from the precipitatedresorcinol mass by decantation.

' the rocess of" purifying and decolori zii ig rOSi IiS, the steps whichcomprise treating a solvent extraction mass from resd inous woodcontaining I0S1I1, P1Il6 011 an other te enes and a relatively volatileliquid by ocarbon immiscible w th resorcinol at low and ordinarytemperatures, with resorcinol at an elevated temperature, cool; ing toprecipitate the resorcinol contaimng dissolved impurities and coloring,matter and separating the rosin solution from the preci itatedresorcinol mass by decantation.

5. n the process of purifying and decolorizing rosin, the steps whichcomprise dissulting mixture substantially to the boiling pointunder'agitation, cooling to a tempera-- comprise ture at which theresorcinol will separate 7 out as a preciptate containing dissolvedimprecippurities and coloring matter and separating 6. The process ofpurifying and decolorizing rosin, which comprises treating a commercialsolvent extraction mass from resinous wood containing rosin, pine oil-'and other terpenes and a light petroleum distillate with a relativelysmall quantity of resorcinol, heating the treated mass to substantiallyboiling temperature under agitation, cooling until the resorcinolseparates out as a preciptate'or crust containing dissolved rosinimpurities and coloring matters, separating the rosin solution from theprecipitated resorcinol and recovering the purified and decolorizedrosin from said rosin solution.

7. The process of purifying and decolorizing rosin, which comprisestreating a petroleum'naphtha extraction mass from resinous wood,containing rosin, pine oil and other terpenes with a relatively smallquantity of resorcinol, heating the treated mass to substantiallyboiling temperature under agitation, cooling until the resorcinolseparates out as a precipitateor crust contaimng dissolved rosinimpurities and coloring matters, separating the rosin solution from thepreci itated resorcinol and recoverlng the puri ed and decolorized rosinfrom sa1d rosin solution.

8. In the process of purifying and decolorizing rosins, the steps whichcompnse heating a rosin dissolved in a volatile liquid hydrocarbon withresorcinol.

9. In the process of purifying and decolorizing rosins, the step oftreating rosin in solution with resorcinol to form a preciptate ofresorcinol containing dissolved rosin impurlties and coloring matter andrecovering the rosin solution from said preciptate.

40 In testimony whereof, we have hereunto subscribed our names.

IVAN GUBELMANN. CLYDE O. HENKE.

